A spectrophotometric method was developed for the determination of Fe(II) and Ni(II). The method was based on the formation of Fe (II), Ni(II) 4-[(4-antipyl azo )]orcinol(APAO) complexes. The complexes have been characterized by spectroscopic methods such as UV-Visible ,FT-IR,molar conductivity measurements ,melting points . The maximum absorbance of complexes are at 469 and 461nm with molar absoptivity of (0.4032×104) and (0.107×105) L.mol-1.cm-1of Fe(II) and Ni(II) respectively .Mole ratio of the complexes which is formed between Fe(II) and Ni(II) with APAO are 1:2 and 1:1 which was calculated by both the mole ratio and continuous variation methods. The absorbance of the complexes obeys Beer΄s law in the concentration range of (0.2-1.5)μg.ml for Fe(II)and (0.4-2.8)μg.ml for Ni(II). The stability constant of the complexes under optimized conditions and at room temperature was (0.14×107 ,0.14×104)L.mol-1 for Fe(II) and Ni(II) respectively .this procedure can be carried out in the presence of many cations and anions in the presence or absence of the masking agents. The method was successfully applied to the determination of Fe(II) ion and Ni(II) in analytical samples.